Rhenium disulfide (ReS2) single crystals are grown by chemical vapor transport technique. Powder X‐ray diffraction analysis of the single crystals shows them to possess ReS2 phase with triclinic unit cell structure. Energy dispersive analysis of X‐rays shows the crystals to be slightly rich in sulfur and deficient in rhenium. The optical bandgap obtained of the as‐grown single crystals is 1.35 eV. The surface morphology study done by scanning electron microscopy shows that the crystal surface to be flat with layer edges, such observation states that the growth mechanism of crystal have happened by mechanism of sheet spreading. The transmission and diffraction mode electron microscopy shows the single crystals to be layered and crystalline, respectively. The Raman peaks are well assigned to the ReS2. Thermogravimetric and differential thermogravimetric analysis shows the single crystals to disintegrate by two steps. The differential thermal analysis shows that the ReS2 possesses initial endothermic followed by exothermic nature for fast heating rates. In case of a slow heating rate of 10 K min−1, other than endothermic followed by exothermic, the end temperature range shows endothermic nature. The kinetic parameters determined by Kissinger relation shows the single‐crystal samples to disintegrate at a higher temperature range.
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